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p-Chlorothiophenol → 6-(4-Chlorophenylsulfanyl)-hexylphthalimide

HRID 2097361
ノート
印刷プレビュー

反応式

HRID 2097361 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.BrCCCCCC[N:16]1[C:20](=[O:21])[C:19]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:18]2[C:17]1=[O:26].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:6][CH2:7][CH2:2][CH2:3][CH2:4][CH2:5][C:25]2[CH:24]=[CH:23][CH:22]=[C:19]3[C:20]([NH:16][C:17](=[O:26])[C:18]=23)=[O:21])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 141120N-(6-Bromohexyl)phthalimide

生成物 1

HCID 866225746-(4-Chlorophenylsulfanyl)-hexylphthalimide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

4-Chlorothiophenol (2.89 g, 20 mmol), N-(6-bromohexyl)-phthalimide (6.20 g, 20 mmol) and K2CO3 (5.53 g, 40 mmol) were suspended in DMF (50 mL) under an atmosphere of argon and stirred at 90° C. for 23 h. The solvent was evaporated under reduced pressure and the residue was partitioned between water (100 mL) and CH2Cl2 (150 mL). The aqueous layer was extracted with CH2Cl2 (2×100 mL), the combined org. layers were dried over Na2SO4, filtered and the solvent was removed under reduced pressure to give the title compound, pure enough for further reactions.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was partitioned between water (100 mL) and CH2Cl2 (150 mL)
  3. extractionThe aqueous layer was extracted with CH2Cl2 (2×100 mL)
  4. dry with materiallayers were dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-2987f79b79ab4f438c4117417e1cc34e
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450348B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート